色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取-气相色谱法测定纺织品中的邻苯二甲酸酯类环境激素

牛增元1,叶曦雯1,房丽萍1,2,薛秋红1,孙忠松1   

  1. 1.Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China; 2.College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003, China
  • 收稿日期:2005-10-20 修回日期:2006-06-19 出版日期:2006-09-30 发布日期:1986-09-25
  • 通讯作者: 叶曦雯

Determination of Phthalic Acid Esters in Textiles by Solid Phase Extraction-Gas Chromatography

NIU Zengyuan1, YE Xiwen1, FANG Liping1,2, XUE Qiuhong1, SUN Zhongsong1   

  1. 1.Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China; 2.College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003, China
  • Received:2005-10-20 Revised:2006-06-19 Online:2006-09-30 Published:1986-09-25
  • Contact: YE Xiwen

PDF

993

被引次数

147

摘要： 采用索氏提取法以正己烷为提取溶剂提取纺织品中的邻苯二甲酸酯类物质(PAEs),以强阴离子交换固相萃取(SPE)小柱净化本底杂质并富集待测物,建立了纺织品中10余种PAEs环境激素的同时测定方法。采用的固相萃取条件为:5 mL正己烷活化、3 mL异辛烷淋洗、2 mL含15%乙酸乙酯的正己烷溶液洗脱。SPE能有效地对提取液进行富集浓缩,同时对纺织物提取液中的杂质净化效果突出。该方法准确可靠,重现性好,在5~100 mg/kg 添加水平,PAEs各化合物的回收率为86.3%~102.7%,相对标准偏差（RSD）一般小于5%。检测的10余种PAEs中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPrP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二戊酯(DAP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)的方法检出限小于1mg/kg,邻苯二甲酸二异壬酯(DINP)与邻苯二甲酸二异癸酯(DIDP）的方法检出限分别为1.74 mg/kg和1.55 mg/kg。

关键词: 纺织品 , 固相萃取, 环境激素, 邻苯二甲酸酯, 气相色谱

Abstract: A method was established for the simultaneous determination of some phthalic acid esters， namely, dimethyl phthalate (DMP), diethyl phthalate (DEP), dipropyl phthalate (DPrP), dibutyl phthalate (DBP), diamyl phthalate (DAP), dihexyl phthalate (DHP), benzyl-n-butyl phthalate (BBP), di-(2-ethylhexyl)phthalate (DEHP), dicyclohexyl phthalate (DCHP), di-n-octyl phthalate (DNOP), diisononyl phthalate (DINP) and diisodecyl phthalate (DIDP) in textiles by solid phase extraction (SPE) coupled with gas chromatography (GC). The phthalic acid esters in textiles were extracted by Soxhlet extraction with hexane, the extracts were then cleaned up and enriched by a strong anion exchange (SAX) SPE cartridge. The parameters affecting the purification efficiency of SPE cartridge, such as solvent conditioning, rinsing, and elution, were studied. Conditioning with 5 mL hexane and rinsing with 3 mL isooctane were proved to be the optimal conditions. Of the several solvent ratios (ethylacetate in hexane) used for selective elution of phthalic acid esters from the SAX SPE cartridge, the 15% (v/v) content for ethylacetate in hexane gave the best result. Under the optimized conditions, the recoveries of phthalic acid esters for spiked standards (n=7) were 86.3%-102.7%, and the relative standard deviations (RSDs) were less than 5%. In this method the detection limits for DMP, DEP, DPrP, DBP, DAP, BBP, DCHP, DEHP, DNOP were all below 1 mg/kg, and the detection limits for DINP and DIDP were 1.74 mg/kg and 1.55 mg/kg respectively. This SPE-GC method is sensitive, accurate and suitable for the analysis of phthalate environmental hormones in textiles.

Key words: environmental hormones, gas chromatography (GC), phthalic acid esters, textile , solid phase extraction (SPE)